Process for recovering gases and vapors from gas mixtures



Feb. 19, 1929. 1,702,311 V. PANTENBURG PROCESS FOR RECOVERING GASES AND VAPORS FROM GAS MIXTURES Filed Jan. 28, 1926 2 Sheets-Sheet 1 Feb. 19, 1929. 1,702,311

v. PANTENBURG rnocsss FOR nncovnnma mas AND vArons .Fnou GAS uxxmas Filed Jan. 2a, 1926 2 Sheets-Sheet 2 Vifa 15-5 Pan fzn [-07 Kb My [man for;

' Patented, Feb. 19, 1929.

N T-so srArEs vrrams aluminum, or rmxroanon-rnn-uanr, ell-1mm,

morass Ion nscovnmo easns Ann varons no! Gas m'rmms.

Application filed January 28, 1986, Serial No. 34,444, and in Germany February 7, 1995.

This invention relates to the treatment ofgas or vapor mixtures for separating thererom one or more of its constituents, by means of ranular adsorption media such as active 5 car on, silica gel,-porous alumina, etc.

Heretofore two methods have been followed. One of these methods, generally referred to as the intermittent method, consists in passing the gaseous mixture through a body of adsorptionmaterial at rest in a chamber. During the adsorption cycle the adsorption material is as a rule cooled to increase its adsorptive capacity while duringthe regeneration cycle heat is applied to it to liberate the adsorbed gases or vapors, as is well understood. This method has considerable disadvantages from the standpoint of thermal efficiency since the adsorption, on the one hand, and regeneration on the other hand, require "90 opposite thermal conditions. \Vhile adsorp- 2 5" this method has as an unavoidable incident the heating and the cooling of the container body, i. e. a transfer to and dissipation of heat energy in the container body which not only 7 represents a net loss but also requires a COOle ing system anda heating system coniderably larger than is required for effecting the required useful heat-transfer from and to the body of adsorption material alone.

It is principally for this reason that the so called continuous method was evolved and developed. This method essentially consistsin transferring the adsorption material, in cyclic order, from an adsor tion chamber to a regeneratin" chamber an back or through a series of adsorption chambersandre enerating chambers alternating with each ot er,

a practice which is fairly represented by the disclosure in the United States patents to Soddy, Nos. 1,422,007 and 1,422,008. While by the continuous method just re ferred to the;mentioned disadvantages incident to the intermittent method are largely avoided and a much, better thermal efliciency is attained, there are various other. disadvantages of different nature which militate against the continuous method and, at times, impede it or even prevent the successful execution thereof. It has been observed that it is extremely diflicult to efl'ect a substantially through the vertical shafts. Some of the in,

terial remains too long in the adsorption space with the result that it becomes ineffective as adsorbent and that gaseous mixtures coming into contact with it in this condition are not acted upon. 'Other portions of the material pass so rapidly through the adsorption space that they are not adsorptively charged to the maximum of the adsorptive capacity and thus pass into theregenerating space with a relatively low gas or vapor charge which again means a lowering of the efiiciency.

Another difliculty incident to the movement of the adsorption material in countercurrent relation to thegaseous mixture treated is presented by the problem of adequately separating the adsorption space from the regenerationspace so that charged adsorption material may continuously pass from the former to the latter while the gaseous mixture is strictly confined to the former. This is absolutely essential when either the adsorption "medium or the gas or vapor to be adsorbed is combustible or explosive in the presence of oxygen at the regeneration temperature, as for instance is the case when the adsorption medium is active carbon or the substance to c be adsorbed is gasoline, and the gaseous mixture contains oxygen, as in the case of a gasoline-air mixture to be separated. The clifficulties in this respect are particularly great "when theoxygen-containing mixture is under a relatively high pressure. For the adsorption operation the higher pressure is parties ularly advantageous, while for regeneration it is undesirable. "It is'therefore a practical desideratum" that the ressures in the adsorption space he maintamed higher than in the regeneration space, which was not practically feasible up to now in connection with the continuous method.

object a method of the kind involved in which theadvantages of thermal efliciency characteristic of the continuous method are full materialized while the corres ondin disa vantages mentioned are entire y avoi ed.

The present invention has as its principal The invention essentially consists in moving the adsorption material in succession through an adsorption space and a regenerating space in endless cycles, in such a Way that the adsorption material during adsorption is at rest and entirely separated from other, parts of the circulation system. It is the prinuniform movement of the adsorption materiak cipal characteristic of the invention that at of an arrangement such as shown in Fig. 1,

including a conveyor system for circulating the adsorptive material; and I I Fig. 5 is a detail in cross-section of an arrangement for discharging adsorptive material from the adsorption vessel.

In the drawings 10 and ll'represent two pressure vessels defining adsorption chambers connected at the bottom by means of conduits 12 and 13, controlled by gates 12 and 13*, respectively, with a regeneration chamber 14. To the latter is connected a gas conduit 14 controlled by a valve ll or the like, forconducting away the gases or vapors set free by the regeneration. At the top the vessels 10 and 11 are connected by means of branches 15 and 16 controlled by means of valve or gates 15 and 16 respectively with a conduit 17 In the bottom portion, the vessels 10 and 11 have conical supports 18 and 19 formed of slats or boards in cascade arrangement resembling louvre shutters, the mouths of which register with the conduits 1'2 and 13, respeo tively. These supports defines surrounding gas spaces 18*? and 19 which are connected through branches 20 and 21, controlled by valve 20 and 21, respectively," to a conduit 22.

The operation is as follows:

2 Assume that the chamber 10 is filled with reactivated or re enerated adsorptive mate'- rial ready to be charged. Valves 20 and 15 v are open while gate 12*.is closed. The gaseous mixture enters thegas s ace 18 preferably tangentially as shown an therefor uniformly fills the circularspace about the sup ort 18 and enters radially in all directions t rough the parallel spgces of the louvre-shutter sup port and thus flows substantially uniformly through the body of the adsorptive material at rest, giving up theconstituent to. be separated, and I the remaining gas flows out through branch 15 into the conduit 17 where it may be collected or disposed of in any desired manner.

Assume alsothat at the same time material adsorptively charged in vessel 11 is simultaneously regenerated in the regenerating chamber 14. Valveslfif and'21 are closed 'while the gate 13 is open. However, in the case when adsorption has-been effected under pressure, the pressure in vessel 11 must first be reduced and equalized with the pressure in the regenerating chamber. To this end are provided conduits 10 and 11- controlled by valves 10 and 11*, respectively, for permitting gas to escape out of vessel 10 or 11, as the case may be, and-thereby reduce the pressure within. The action in the regenerating chamber itself may be in accordance with the usual or any preferred practice. Thus,

regeneration can be efiected, for instance, by passing supreheated steam through the material or by indirectly heating it or by a combination of both methods. In the case of indirect application of heat, the regenerating chamber may be advantageously provided with a heating jacket 14. After regeneration the material is transferred back to the vessel 11 after being cooled in the usual way by pass-. ing it first through a cooler 23. The regenerated material is transferred by means of any suitable conveyor 9 to a ho per 9' and re enter's vessel 11 through the 1ntake ,24, the chamber 10 having a similar intake 24.

The charged material in vessel 10 is then regenerated, while the regenerated material in vessel 11 is charged. The regenerated material is returned to the vessel 10 through the intake 24 ;The operation is thus continued by alternately charging material while at rest material in the regenerating vessel 14.

The transfer of the material from the vessel 10 or 11 to the regenerating chamber and then back' to the vessel 10 or 11 may be effected intermittently .;or continuously.

In the latter case, one of the vessels 10 or ll'is connected t6 the gas conduit 22, while from the other the charged material is passed in a continuous operation to the regenerator, which is constantly filled with material. The

. regenerated material is likewise continuously withdrawn from the bottom of the regeneratingchamber 14 and transferred to that adsorber vessel from which the regenerator receives the'charged material.- When the transfer has been completed and the particular adsorber vessel is filled with regenerated material, the cycle is reversed. The material is thus continuously moving through and out of the regenerating vessel.

In order to prevent a mixing between the degenerated material being fed into the adsorbervessel and the material being discharged from it, it is necessary in that case to provide means for efl'ecting a uniform downward movement of the material in the adsorber vessel. As an efi'ective means to that end, I provide a plurality of round or polygonal disk-like bodies 25 of different sides and in such relative spacing that the incoming material and the outgoing material in their downward course define a substantially constant contact surface and do not in one of the vessels 10, 11 and regenerating mingle. Instead of plates 25 in the relation described, similar plates 26 may be superposed in staggered relation. For the sake of illustration I have shown both arrangements in the same apparatus. .In Fig. 5 are shown in 'detaail-these arrangements as well as the arrangements vby means of which the gas or vapor mixtures are introduced for subjection to the adsorptive treatment. 26 is a centrally located circular plate beneath which are arranged a number of annular plates 26 of difl'erentdiamters and verticall from each other as shown. These p ates as a a whole constitute a kind of upwardly tapering cone, and the adsorptive material flows over the separated annular plates according to its natural slope towards the periphery of the vessel. From the periphery of the vessel, the adsorptive material flows over the annular sheets 19 arranged in a hopper-like formation, and is directed into the exit 13. As shownin Figs. 1 and 2, the gas is introduced into the space 19 surrounding this hopper. From this space "the gas or vapors is or are passed through the slits of'the sheets which form this exit hopper and through the layer of adsorptive material into the hollow space which lies underneath the annular plate 26 From this space the gas streams through the vertical spaces of the horizontally arranged annular plates into themain body of adsorptive material, and after passing therethrough flows into the exit pipe at the top of the adsorbing chamber. Any other instrumentality for regulating the flow of the material in the adsorber vessels maybe used.

Means for regulating the flow of the material may be obviated by employing three adsorber vessels 27, 28 and 29, as shown in Fig. 3, where 30 represents the common regenerating chamber connected to the adsorber vessels by the conduits 31, 32 and 33, controlled by valves 31, 32 and 33, respectively. For carrying ofi'the gases or vapors liberated during regeneration, there is provided a conduit 30 controlled by a valve 30 or the like. A common gas feed main 34 is connected'with the adsorbers by valved branches 34, 34" and 34, while the topsof the adsorbers are connected by valved branches 35, 35" and 35 to a con duit 35. Thevessels 27, 28 and 29 are provided with conduits 27; 28 and 29 controlled by valves 27, 28" and 29*, respectively, for

releasing the pressure within any one of the vessels. I

The operation in this case is so conducted that one of the adsorbers is always connected to the gas main, while from one of the other two adsorbers char ed material flows into the regenerating vesse and material from the regenerating vessel movesto. the third adsorber. As soonas the second adsorber is empty and the third adsorber is filled, the s stream is passed into the latter while, the

adsorber 1s emptied and the second spaced,

adsorberis beingfilled. This arrangement precludes the possibility of a mixing of charged material with regenerated material.

At any rate, the adsorption operation is carried out with the material at rest and the adsorption, on the one hand, and the re eneration, on the other hand, may be carrie out under entirely different pressures.-

The two forms of apparatus diagrammatically referred to, are of course not the only apparatus available for carrying out the invention. However, I found that they are particularly suited for the purposes of the invention.

The arrangement shown in Fi 3 has also particular utility in cases where t ration is carried out under high pressure. In such cases, after the adsorption operation in one of the adsorbers is com leted, the gas pressure therein must be gra ually reduced to the pressure in the regenerator. A This re- 6 gas sepaductionmust be gradual since otherwise .ad

sorbent material would be carried' out with the escaping gas. The rate at which gas should be allowed to escapeghowever, would be too slow to be practical. For this reason a larger number :of adsorbers facilitates the operation, inasmuch as in one of the adsorbsorption under high compression, the a vantages are not limited thereto.

I claim: 1. Apparatus for separating gaseous mixtures by adsorption, com rising a lurality' of adsorption chambers aving eac an intake and an outlet for the adsorption material,

a re aerating chamber, valve controlled connections between the latter and the outlets of the separate adsorption chambers and separate 'valve-eontrolled gas inlets and outlets for theadsorption chambers.

2. Apparatus according [to claim 1, ;in which "each adsorption chamber hasnear its bottom an annular gas chamber separated from the adsorption space by an apertured artition, the gas inlet ioreach adsor tion g) amberbeing connectedto the saidgasc amer. a I

3. Apparatus according to .claim 1, in which each adsorption chamberhas near its bottom an apertured funnel-shaped partition defin' an annular gas chamber separated from e adsorption space bythe partition,

i the gas inlet for each adsorption chamber be ing connected to the said gas chamber.

4. Apparatus according to claim 1, in I partition, the gas inlet for each adsorption chamber being connected to the said gas chamber and entering it substantially tangentially.

5.Apparatus according to claim 1,'in

which each adsorption chamber is provided with means for causing the adsorption material, to move substantially uniformly from top to bottom.- Y

6. Apparatus according to claim 1,' in which each adsorption chamber is provided with a plurality of disk-like bodies disposed in spaced relation so as to cause the adsorption material to move substantially uniformly from top to bottom.

a 7. Process for the separation of substances from gas, vapor or gas-vapor mixtures, by adsorption, characterized thereby that the substance to be separated is adsorbed alternately under high pressure in several adsorption chambers by suitable adsorption material and that as soon as the adsorption'material has taken up a sufficient quantity of the substance to be separated. the pressure in the adsorption space is diminished whereupon the adsorption material is conducted into a separate common heating chamber, and there, at lower pressure, the adsorptively held materials are driven out, so that the adsorption material becomes useful. again for the adsorption'treatment of gas, vapor or gas-vapor mixtures 7 r 1 8. Prdcess for the separation of substances from gas, vapor or gas-vapor mixtures, adsorption, characterized thereby that the substance to be separated-is adsorbed alter tion chambers by suitable adsorption mate;-

'nately underhigh'pressure'in several adsorprial, While maintaining' the adsorptionjmate rial at rest therein, and that as soonas the adsorption material'has taken up-a sutfic'ient quantity of the substance to be separated the pressure in the adsorption space is diminished whereuponthe adsorption material is contively held materials are driven out, so that the adsorption material becomes useful again for the adsorption treatment of gas, vapor or gas-vapor mixtures.-

9. Process 'forrthe separation of substances from gas, vaporor gas-vapor mixtures by .VITALIS PANTENBURG.

ducted into a separate common heating cba m i her, and there, at lower "pressure, the adsorp- 

